al Bureau of Standards

TECHNICAL

m ^fMfe % m

417

Spectral Emission Properties of

N6S Standard Phosphor Samples

Under Photo-Excitation

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U.S. DEPARTMENT OF COMMERCE

National Bureau of Standards
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UNITED STATES DEPARTMENT OF COMMERCE

C. R. Smith, Secretary

NATIONAL BUREAU OF STANDARDS • A. V. Astin, Director

NBS TECHNICAL NOTE 417

ISSUED MARCH 1968

Spectral Emission Properties of

NBS Standard Phosphor Samples

Under Photo-Excitation

Carl F. Shelton

Metrology Division

Institute for Basic Standards

National Bureau of Standards

Washington, D.C. 20234

NBS Technical Notes are designed to supplement the Bureau's regular publications program. They provide a means for making available scientific data that are of transient or limited interest. Technical Notes may be

listed or referred to in the open literature.

For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, D.C, 20402

Price 25 cents.
Contents

Page

1. INTRODUCTION 1

2. MEASUREMENT TECHNIQUE 1

3. COMPUTER CORRECTION OF DATA 3

3. 1 Results 5

4. RELATIVE QUANTUM EFFICIENCY 26

REFERENCES 29

ii
SPECTRAL EMISSION PROPERTIES OF NBS STANDARD

PHOSPHOR SAMPLES UNDER PHOTO-EXCITATION

Carl F. Shelton*

The photo-excitation spectral emission properties

of 10 of the 14 NBS standard phosphor samples have been

determined. Pressed tablets of the phosphors were excited by radiation from a mercury arc lamp, passing

through a narrow band-pass filter to obtain either 2537A

or 3650A excitation. The measurement system is described,

correction of the data is discussed, and the spectral

emission data are presented. Relative quantum efficiencies were calculated. The results are compared with

measurements reported by two other laboratories.

Key Words: Phosphors, photo-excitation, photoluminescence, spectral emission, spectral radiometry, standard

phosphor samples.

1. Introduction

The spectral emission properties of ten NBS standard phosphor samples

under ultraviolet excitation have been measured. The phosphors and the

exciting radiation used are listed in Table I. The relative quantum efficiencies of the 2537A excited phosphors were calculated relative to magnesium

tungstate from the data obtained.

The purpose of this report is to describe the measurement technique

used, to discuss a computer program written to reduce the raw data, and to

present the results obtained. k2.Measurement Technique

Measurements of the relative spectral emission of the phosphor samples

under photo-excitation were made with the equipment shown in Figure 1. The

phosphor powder sample to be measured was placed in a small cup made of

aluminum (1.25 inches in diameter and approximately 0.04 inch deep) and

pressed level by using a spatula. This phosphor plaque was then placed on a turret sample holder mounted horizontally in front of the monochromator

which was mounted vertically.

A 4-watt low-pressure mercury-arc lamp (germicidal) was used as source

for 2537A excitation with a filter (Corning No. 9863) in front of the lamp

to block the mercury lines in the visible region. A 100-watt high-pressure

mercury-arc lamp with a narrow-band-pass filter centered at 3650A, in front

*Research Associate from the International Business Machines Corporation at

the National Bureau of Standards, 1967.
TABLE I

Sample

No.

NBS Standard Sample Pho

Measurement

Excitation (A) Phosphor Descr

3650 Zinc Sulfide

ZnS:Ag

sphors

iption Use

1020 Blue Component of

P-4 Cathode Ray Tube

(CRT) Phosphor

1021 2537 Zinc Silicate

Zn-SiO, :Mn

2 4

P-l CRT Phosphor

1022 3650 Zinc Sulfide

ZnS : Cu

P-2 CRT Phosphor

1023

1024

1025

1026

1027

1028

1029

1030

1031

1032

1033

3650

3650

.... (i)

2537 ^

2537

2537

2537

- —(2)

2537

- —(3)

- —(3)

Zinc -Cadmium Sulfide

ZnCdS:Ag

Zinc-Cadmium Sulfide

ZnCdS:Cu

Zinc Phosphate

Zn

3

(P04

) 2

:Mn

Calcium Tungstate

CaWO, :Pb

4

Magnesium Tungstate

MgW0

4

Zinc Silicate

Zn-SiO, :Mn

2 4

Calcium Silicate

CaSi0

3

:Pb,Mn

Magnesium Arsenate

(MgO) x (As o c ) :Mn ° x 2 5 y

Calcium Halophosphate

3Ca o (P0,) .Ca(F,Cl) :Sb,Mn

3 4

Barium Silicate

BaSi

2

:Pb

Calcium Phosphate

Ca

3 (P04

) 2 :Tl

Yellow Component of

P-4 CRT Phosphor

Orange Component of

P-14 CRT Phosphor

Red Component of

P-22 CRT Phosphor

CRT, Lamps

CRT, Lamps

Lamps

Lamps

Lamps

Lamps

Lamps (UV)

Lamps (UV)

(1) Would not emit under 2537A or 3650A excitation

(2) Fine emission structure not resolved with 5A pass band of monochromator used; results not reported

(3) Not measured.
of the lamp, was used as a source of 3650A excitation. The output of

the monochrotnator was measured by using a photomultiplier tube (PMT)

with an S-20 photocathode (Dumont EM2433), an amplifier or a picoammeter,

and a digital voltmeter as shown in Figure 1.

VOLTMETER

AMP]LIFIER |

HV

SUPPLY \1 1 DUAL GRATING

MONOCHROMATOR

COLOR TEMP L

AND HOUSING

<\MP ^ >

i

i

Frun

J| EXCITATION SOURCE AND HOUSING

' FILTER

.....sna 1 TURRET SAMPLE HOLDER

Figure 1 Spectral Measurement Equipment

In order to calibrate the monochrotnator and PMT combination! its relative

spectral sensitivity was measured by using an NBS color temperature standard

operated at a color temperature of 2854K. A USP grade barium sulfate (standard

reflector) plaque was placed on the turret sample holder so that it could be

rotated into position in front of the entrance slit of the monochromator. The

spectral radiant flux of the color temperature standard, as diffusely reflected

by the plaque, was used to calibrate the equipment*

A measurement of the phosphor sample consisted of setting the monochromator

at a 'particular wavelength (scale readable to three places), and recording the

digital voltage reading; first, with the color temperature lamp and the BaSO,

plaque; and second, with the excitation source and the phosphor sample in front

of the entrance slit. Both lamps were housed and shuttered such that they

could be left on continuously during a data run and used independently* The

wavelength scale on the monochromator was verified by using the mercury lines

in the low pressure excitation source*

3. Computer Correction of Data

A computer program was used to calculate the relative spectral sensitivity

of the instrument for each run and to apply calibration corrections to the

data obtained in order to obtain the relative spectral distribution of the

phosphor photo-luminescence for each data run* The corrected phosphor

relative radiant energy distribution curves for several independent runs were

then averaged over the number of runs to provide an average curve for each

phosphor measured*
The following quantities are de* fined:

N = Number of data runs for each phosphor

X. = Wavelength value: j =1, . .., 20

S.(\.) = Relative sensitivity of instrument for the i-th data run

i J i = 1, . .

. , N

C.(X,.) = Digital voltage reading when using color temperature lamp

-* and BaSO, plaque for the i-th data run at the j-th wavelength

value

L(\.) = Relative spectral luminance of BaSO, plaque when irradiated

-' by color temperature standard (2854k).

D.(\.) = Digital voltage reading when using excitation source and

i J phosphor plaque.

Thus, since C.(\.) is by definition

C

l (X

j

) = S

i

(X

j

} L(V' (1)

the relative spectral sensitivity for the i-th data run is therefore

C (X. > W= -iotr (2)

also byj definition,> D.(X.) = S.(X.) ?A\.) (3)

i J i J i J whe re

P.(\.) = Relative radiant energy distribution of the phosphor for i-th

. data run. D.(\.) D.(\.) L(X.)

Therefore, * (X > = f^ = * C ] (XJ <4>

i j i J

and the normalized distribution curve is given by,

NP,(X ) = ^-^» (5)

J

i,Max

where:

P. = Maximum value of P.(X.) for j = 1,...,20

Max 1 J

and the average relative energy distribution over the N data runs for each

phosphor is finally „

i=i 1 r

ave v y n
3.1. Results

The relative energy distribution curves obtained for the ten phosphors

measured are shown in figures 2 to 11. Each figure is followed by its

computer output data, in Tables 2 to 11, showing the tabular values for each

curve. The average curve for each phosphor is plotted and the tabular values

are given on each curve. The tabular values shown are 95% confidence interval estimates of the true mean, calculated as:

i

X ± T W

n

where: w = range (maximum value minus minimum value) n = sample size x = computed mean of sample

and values of t are given in Table 8c(l), page 408, of Ref. 5.

The relative energy distribution curves obtained for Sample Nos. 1020,

1022, 1023 and 1024 with photo-excitation are compared with data obtained

with cathode-ray excitation by Bril (Ref. 2). Sample 1022 is a P-2 phosphor

and the JEDEC P-2 data (Ref 3) is compared with the results obtained with

photo-excitation

.

The relative energy distribution curves obtained for Sample Nos. 1021

and 1026 with 2537 A excitation are 'compared with results obtained by Bril

(Ref 1) also with 2537 A excitation. While Sample No. 1021 compares very

closely with Bril's data, Sample No. 1026 shows some differences. Sample Nos.

1026 and 1029 have been compared with data obtained in 1961 by Dr. Frank J. Studer at the Nela Park Laboratory of the General Electric Company (now at

NBS). The two sets of data are in close agreement. Since Sample No. 1021 is

a P-l phosphor, the JEDEC P-l curve is also plotted from Ref, 3.

The difference shown in comparing the results obtained with photo- and

cathode-ray excitation are the same order of magnitude as the differences

noted above obtained for Sample No. 1026 from data obtained with only photoexcitation, e.g., compare results for Sample No. 1024 where the results of

photo and cathode ray excitation are shown, with Sample No. 1026. One might

therefore hypothesize that the spectral emission curves are independent of

the excitation used, but this hypothesis requires further investigation.

The tabular results show the repeatability of the measurements. In

general, the results obtained with the low-pressure mercury-arc lamp (2537 A

excitation) are more repeatable than those obtained with the high-pressure

lamp (3650A excitation) because of greater fluctuations of the output of the

latter lamp.

Other measurement problems and sources of uncertainty include the

low resolution of the wavelength scale on the monochromator (readable to

only three places), the incomplete blocking of the mercury lines by the filter

(preventing accurate readings near 4000 A with 2537 A excitation source), and

the variations in the physical repositioning of the sample with the turret

mount between data points.

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The 45°-0° spectral reflectance factor of the BaSO. plaque was assumed

constant over the wavelength range of interest for each phosphor and the re- lative spectral emission for a blackbody at 2854°K was used for L(A,.) in all

calculations involved in correcting the data. The absolute spectral reflectance of USP grade (unpublished data) BaSO, is shown in Figure 12. The 45°-0°

spectral reflectance factor of the plaque was assumed to be equal to its

spectral reflectance.

4. Relative Quantum Efficiency

The relative quantum efficiencies of the 2537 A excited phosphor

samples have been calculated from the scale factors used with a picoammeter

during the measurements. The method of calculation is as follows: define

f = scale factor

then the calibrated spectral energy distribution is

E(X) = f P (X)

where P(A-) is the average curve obtained for each phosphor. Thus, since

p u nc

E - hv = T >

the number of quanta of luminescence is given by,

til?

J hee he

X

XF(X)dX .

Since the calculated quantum efficiencies of the samples will be referred

to MgWO, , we compute the number of quanta emitted by it as

fMgW0

4

QMgWO,

= he J X P

MgWO, (X)dX .

Finally the relative quantum efficiency of each sample is given by,

e = Relative Q.E. =

f J

X7(X)dX

^W0

4 W J

^^

or for ease of calculation from the data,

f

2 S X. P(\.)

1-1 J J e =

20

fMIin E X.?(X.) MgWO j j 4 J=i

26
Figure 12. Spectral Reflectance of Barium Sulfate

27
The following results were obtained with the quantum efficiency of MgWO,

normalized to unity.

RELATIVE QUANTUM EFFICIENCIES

OF 2537 A EXCITED SAMPLES

Sample No. Per Bril (Ref 1)

1021

1026

1027 (M WO.)

g 4 1028

1029

1031

.66 .83

.86 .89

1.00 1.00

.86 .81

.85 .81

.82 .84

28
REFERENCES

3.

6.

A. Bril and W. Hoekstra, "Efficiencies of Phosphors for Short -Wave Ultraviolet Excitation," Philip Res. Repts. J.6, 356-370, (1961).

A. Bril, "Absolute Efficiencies of Phosphors with Ultra-Violet and

Cathode-Ray Excitation," Kallman and Sprunch, Luminescence of Organics

and Inorganic Materials, Wiley, 1962.

"Opitcal Characteristics of Cathode Ray Tube Screens," JEDEC Publication

No. 16A, JEDEC Electron Tube Council, January 1966.

F. J. Studer, "Measurement of Quantum Efficiency" General Electric Research

Laboratory Memo Report, November P-207, November 1959.

Dixon and Massey, "Introduction to Statistical Analysis", McGraw-Hill,

1957 (page 408).

Goebel, Caldwell, and Hammond, Journal of the Optical Society of America

56, 783-788, (1966).

29

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